Process of making alkali-metal oxids.



UNITED STATES PATENT OFFICE.

GEORG WILHELM MEISER, OF LUDWIGSHAFEN-ON-THE-RHINE, GER- MANY, ASSIGNOR TO BADISGHE ANILIN UND SODA FABRIK, OF LUDWIGSHAF EN-ON-THE-RHIN E, GERMANY.

Specification of Letters Patent.

Patented 14, 1906.

Application filed October 14, 1902. Serial No. 127309.

To all whom it may concern.-

Be it known that I, GEORG WILHELM MEI- sER, doctor of philosophy and chemist, a subect of the Kin of Bavaria, residing at Ludwigshafen-on-t e-Rhine, in the Kingdom of Bavaria, Empire of Germany, have invented new and useful Improvements in Processes of Making Alkali-Metal Oxids, of which the following is a specification.

It has hitherto been impossible to prepare pure alkali-metal oxid having the composition represented by the formula Na O or K 0. All attempts to prepare such oxids have resulted in lmpure products. For instance, Beketof was only able to prepare a product containing thirty to sixty-slx per cent. of K 0. (See Berichte 14, pa e 2058.) Further, de Fouorand on account of the difficult he found in preparing pure sodium oxid ad to-be content with a mixture of Na,0,and Na O. (See Comptes Rendus,Vol. 128, page 1449; also,Ber., Vol. XII,page 856; Vol. XVI, age 1854; Vol. XX, part 3,page 190.) In act, so defective and uncertain has been our knowledge of this subject that in recent times it has been doubted whether such oxids exist at all. (See Erdmann, Lehrbuch der Anorgan'ischen Chemie, third edition, 1902, page 516.) Further, the means hitherto em loyed in the attempts to obtain these oxi s have necessitated the prolonged application of extraneous heat, and the vessels in which such reactions were car ried out have been strongly attacked.

The present invention consists in preparing alkali-metal oxids which for practical purposes are pure without the emplo ment of extraneous heat to any considerab e extent.

According to this invention alkali-metal powder is intimately mixed with alkalimetal superoxid and the components are caused to react together. Such a mixture is conveniently obtained by grindin an alkali metal with a superoxid of an alksfii metal. On exposure to air or b local warming-for example, by means 0 a match or hot wire-the mixture ignites. The mass then becomes red-hot, because of the heat of the reaction and without the aid of extraneous heat, and an alkali-metal oxid results. The reaction (which is preferably performed in the absence of air or oxygen or in the presence of an indifierent gas, so as to avoid the re-i'ormation of alkali superoxid) takes place so quickly that ractically no corrosion of the vessel in which it occurs can take lace, and during the ignition the walls and lIottom of the vessel may be cooled to further prevent the possibility of an such action of the materials'on them as wouId render the product im ure.

That the new products are practica ly pure and may be re resented by the empirical formula R 0 (w ere R represents an atom of an alkali metal, such as potassium or sodium) can easily be shown by analysis-for example, by carefully treating such product with water and titrating it with standard acid. Of course if a mixture of oxids R,,O (say of sodium and potassium oxid) is being examined the proportion of the constituent metals must-be allowed for in the well-known manner. The new products are fitwithout any further treatment for application in the manufacture of indigo by use in the caustic alkaline melt containing phenyl glycocoll.

The following exam le will serve to further illustrate the nature 0 this invention; but, as will be understood from the foregoing description of the scope of the invention, it is not confined to the precise conditions, apparatus, or materials specifically named in this example. The parts are by weight:

Example: Grind together in a ball-mill thirty-nine (39) parts of sodium eroxid and twenty-three (23) parts of meta lic sodium. If air be excluded, no reaction, such as ignition of the sodium, takes place, and a mixture of sodium powder and powdered sodium peroxid results. Ignite the mixture obtained either in the mill itself or after havin transferred the mixture to another vesse. The i nition can be effected by locally warming the mass, which then burns violently and melts. Should a part of the material in spite of the violent reaction remain unconverted, grind up the reaction mass again and heat it or from about one-quarter to half to an hour, so that the powder shrinks together to a white compact mass. It then forms practically pure sodium oxid. In a similarmanner potassium oxid can be prepared from potassium superoxid and meta 'c potassium.

There is claimed-- 1. The process for the production of alkalimetal oxids which consists inrpix'ing together its ownreaction while cooling the vessel in the alkali metal with an alkal -metal peroxid which the reaction occurs.

and causing the resultant mlxture to react In testimony whereof I have hereunto set and combine substantially under the heat of my hand in the presence of two subscribing 5 its ow rlnhreactiomf h d f lkal wltnesses.

2. e rocess ort epro uctlono a imetal axis which consistsinmixing together GEORG WILHELM E the alkali metal with an alkali-metal peroxid Witnesses: and causing the resultant mixture to react ERNEST F. EHRHARDT lo and combine substantially under the heat of JACOB ADRIAN. 

